O presente trabalho é uma contribuição para o esclarecimento e a quantificação das influências na deformabilidade e na capacidade portante de elementos unidimensionais de concreto armado em solicitação plana, decorrentes da não-linearidade física dos materiais concreto e aço, bem como da fissuração e do enrijecimento da armadura tracionada, também na sua fase plástica. Para aplicações práticas determinam-se a rigidez à flexão e a capacidade de rotação plástica dos elementos estruturais, o que permite limitar com mais precisão e coerência a demanda de rotação plástica obtida na análise. De início, descrevem-se os comportamentos não-lineares do concreto e do aço, aplicando-se conceitos da Mecânica da Fratura, bem como a atuação conjunta destes materiais, sob os aspectos de aderência e de fissuração. O núcleo deste trabalho concentra-se na obtenção do diagrama momento-curvatura e dos seus pontos principais, e na subseqüente determinação da capacidade de rotação plástica dos mencionados elementos. Consideram-se as seções geradas a partir da seção duplo T assimétrico, com várias camadas de armadura, sujeitas à flexão composta normal. Com dados deste diagrama e através do modelo da viga equivalente simétrica, posteriormente estendido à viga equivalente assimétrica e às vigas contínuas de pórticos planos, determina-se a capacidade de rotação plástica, considerando-se nesta suas múltiplas influências. Por fim, comparam-se os resultados teóricos e experimentais da capacidade de rotação plástica, e resumem-se as principais conclusões encontradas e os pontos que exigem subseqüente desenvolvimento. / The present study is a contribution to the enlightenment and evaluation of the influences on deformability and load carrying capacity of one-dimensional elements of reinforced concrete subject to in-plane loading, arisen from the constitutive non-linearity of concrete and steel, as well as from the concrete cracking and the tension stiffening of the reinforcement, prior and after yielding. For practical applications, the flexural rigidity and the plastic rotation capacity of structural elements are determined, which makes it possible to limit, more precisely and coherently, the plastic rotation demand coming from the analysis. Firstly, the non-linear behaviors of concrete and steel are described, applying concepts of Fracture Mechanics, and then the joint action of both materials concerning bond and cracking is studied. The core of this study lies on obtaining the bending moment-curvature diagram, specially its main points, and on the subsequent determination of the plastic rotation capacity of the aforementioned elements. The cross-sections generated from an asymmetric double T cross-section are considered, with several layers of reinforcement, acted upon simple or combined bending about one principal axis. With data based on this diagram and through the model of equivalent symmetric beam, later extended to equivalent asymmetric beam and to continuous beams of plane frames, the plastic rotation capacity is determined, considering its multiple influences. Finally, theoretical and experimental results of plastic rotation capacity are compared, and the main conclusions and points in need of subsequent development are summarized.

O objetivo do trabalho foi avaliar a resistência à flexão, microdureza e grau de conversão de 9 resinas compostas para uso indireto: Solidex (Sl), Epricord (Ep), Belleglass (Be), Signum (Sg), Sinfony (Sy), Tescera (Te), Cristobal (Cr), Targis (Ta) e Adoro (Ad); e uma resina para uso direto como controle, Esthet X (Et), em função da cor: esmalte (E), dentina (D) e translúcido (T). O teste de resistência à flexão (n=15) obedeceu ao método dos três pontos (Kratos) e, após a obtenção dos valores de carga, os corpos de prova fraturados eram posicionados em fita matriz de poliéster e fixados com resina quimicamente polimerizável (Adaptic) no paralelômetro. Em seguida, os corpos de prova eram levados ao microdurômetro (Shimadzu), para obtenção dos valores de microdureza Knoop (n=15), através da aplicação de uma carga de 50gramas por 30 segundos. Para o grau de conversão (n=3), os corpos eram construídos na mesma matriz usada para resistência à flexão, e posicionados em frente ao feixe de infravermelho do espectrofotômetro Raman (Bruker RFS 100/S - 64 scans) para leitura do grau de conversão. A análise de Variância e teste de Tukey foram usados para tratamento dos dados obtidos. A partir dos resultados, chegou-se às seguintes conclusões: 1. Resistência à flexão: O ranqueamento variou em função da cor e as resinas Cr, Sy, Be e Ta tiveram valores de resistência flexural estatisticamente superiores aos dos outros materiais. Os piores materiais foram o Ep, Sg e Sl. A cor não mostrou diferenças significantes (p=12), mas a interação (p<0,0001) e o material (p<0,0001) mostraram. Dois grupos intermediários entre estes foram encontrados. Um deles com valores muito próximos ao grupo com maiores médias de resistência flexural, os quais se encontram os materiais, Et e Te e, um terceiro grupo foi composto pelo material Ad. 2. Microdureza: As resinas Te > Cr > Be > Et, se destacaram com os maiores valores de dureza, (em ordem decrescente de valores de dureza, e com diferenças significantes entre elas). Os piores valores foram obtidos por Ad e Sy com diferenças significantes entre eles. Ep, Sg, Sl e Ta constituíram um grupo com valores intermediários. Portanto, o material (p<0,0001) e a interação (p<0,0001), obtiveram diferenças significantes. Em relação à cor (p<0,0002), a cor indicada para esmalte apresentou valores estatisticamente inferiores do que dentina e translúcido, e deve ser atribuída aos baixos valores em esmalte, em relação a outras cores do material Te. 3. Grau de conversão: Os maiores valores foram obtidos pelo material Te > Be > e = Cr > ou = Sy = Ad. Os materiais Ep e Ta apresentaram valores de grau de conversão logo abaixo destes materiais, e os piores valores de grau de conversão foram mensurados nos materiais Sg, Et e Sl, com diferenças estatisticamente significantes entre eles. Em relação à cor (p<0,0001), a cor indicada como translúcido apresentou valores estatisticamente superiores aos das duas outras cores. Estes resultados são devido aos altos valores apresentados pelos materiais Sy e Ep. Também tiveram valores significantemente diferentes o material (p<0,001) e a interação (p<0,0001). / Objectives: To characterize nine laboratory-processed composite systems (Adoro [Ad], Belleglass [Be], Cristobal [Cr], Epricord [Ep], Sinfony [Sy], Signum [Sg], Solidex [Si], Targis [Ta] andTescera [Te], ) and one composite for direct placement (Esthet-X [Et]) in terms of particle-size distribution and to compare the flexural strength (FS), Knoop hardness (KH) and degree of conversion (DC) of these composites. Materials and methods: Approximately 5 g of composite paste were dissolved in acetone pro analysi, mixed and centrifuged for 30 min at 3000 rpm. The remaining filler particles were dried (37 °C/12 h) and ultrasonically agitated. A computer-controlled apparatus using laser-diffraction technology was used to determine particle size distribution. Specimens (10 x 2 x 1 mm) were fractured with a 3-point bending test (n=15). KH was measured on fragments obtained after the flexural test (25g/30s). Raman spectra of both unpolymerized and polymerized resins were measured at room temperature in the backscattering geometry using the FT-Raman spectrometer. FS, KH and DC data were analyzed with one-way ANOVA and Tukey\'s post-hoc test (?=0.05). Results: The range of particle sizes was dramatically different for each composite. The composite Et showed the narrowest range of particle size while Sg showed the widest range. The highest DC means were observed for Te, Be and Cr. The lowest means were observed for Sg, Et and Si. Cr, Sy and Ta showed the highest FS values, while Ep, Sg and Si showed the lowest FS values. Te, Cr, Be and Et showed the highest KH means, while Ad and Sy the lowest. Conclusions: The composites Te, Cr and Be showed the best performance in all methods evaluated. On the other hand, the indirect composites Ep, Sg and Si demonstrated the worst performance.

Resumo: Neste estudo avaliou-se a influência do tratamento de superfície para cimentação na resistência à flexão de 4 pontos de zircônia tetragonal policristalina estabilizada por óxido de ítrio (Y-TZP). Por meio de blocos pré-sinterizados de Y-TZP (InCeram 2000 YZ Cubes, Vita Zahnfabrik) foram confeccionadas 120 barras (20mm x 4mm x 1,2mm) de acordo com a norma ISO 6872:2008 e aleatoriamente divididas em 4 grupos: Grupo 1: silicatização (Cojet 30 μm) (n=29); Grupo 2: jateamento com óxido de alumínio (44 μm) (n=29); Grupo 3: ponta diamantada de granulação extra-fina (30 μm) (n=27); Grupo 4: (controle) sem tratamento de superfície (n=29). Em seguida, todas as amostras foram submetidas ao ensaio de flexão de 4 pontos (imersos em água destilada à 370C) em máquina de ensaio universal com velocidade de 0,5 mm/min até o rompimento das mesmas. A análise de difração de raios-X foi utilizada para determinar a transformação de fase. A microestrutura da Y-TZP e o padrão de tratamento de superfície foram analisados por meio de perfilometria óptica e microscopia eletrônica de varredura. Os dados de resistência à flexão foram estatisticamente analisados por meio de ANOVA 1-fator, teste de Tukey HSD (α=0,05) e Weibull (m=módulo; σ0=resistência característica). As médias±desvio-padrão (MPa) foram os seguintes: G1:1207,1±229,7a; G2: 1369,7±272,3a; G3: 874,4±365,4b e G4: 1196,2±284,2a. Os valores de (m) e (σ0) foram: G1: 6,0 e 1300,28; G2: 5,9 e 1477,88; G3: 2,6 e 985,901 e G4: 4,5 e 1308,12. Concluiu-se que a utilização de pontas diamantadas de granulação extra-fina deve ser evitada nos procedimentos prévios à cimentação resinosa de Y-TZP / Abstract: This study evaluated the influence of surface treatment on 4-point bending test of yttrium stabilized policristaline tetragonal zirconia (Y-TZP). From Y-TZP blocks (InCeram 2000 YZ Cubes, Vita Zahnfabrik) were obtained 120 bars (20mm×4mm×1.2mm) according to norm ISO 6872:2008 and randomly divided in 4 groups: Group 1: silicatization (Cojet 30 μm) (n=29); Group 2: sandblasting with aluminium oxide (44 μm) (n=29); Group 3: fine coarse diamond bur (30 μm) (n=27); Group 4: (control) without surface treatment (n=29). As follow, all samples were submitted to the 4-point bending test (immersed in distilled water at 370C) in an universal testing machine with cross-head speed of 0.5 mm/min until the rupture of the samples. X-ray diffraction analysis was utilized to quantify the monoclinic phase. The microstructure of Y-TZP and pattern of surface treatment were analyzed by optic profilometer and scanning electron microscopy. The data of flexural strength (σ4p) were statistically analyzed by 1-factor ANOVA, Tukey HSD (α= 0.05) and Weibull (m= modulus, σ0 = characteristic strength). The mean±standard deviation (MPa) were the following: G1:1207.1±229.7a; G2: 1369.7±272.3a; G3: 874.4±365.4b and G4: 1196.2±284.2a. The values of (m) and (σ0) were: G1: 6.0 and 1300.28; G2: 5.9 and 1477.88; G3: 2.6 and 985.901 and G4: 4.5 and 1308.12. It was concluded that silicatization and sandblasting increased the flexural strength of Y-TZP, diminished the roughness of surface and present higher reliability for cementation of Y-TZP restorations / Orientador: Estevão Tomomitsu Kimpara / Coorientador: Mutlu Özcan / Banca: Paulo Francisco César / Banca: Alfredo Mikail Melo Mesquita / Banca: Rubens Nisie Tango / Banca: Fernando Eidi Takahashi / Doutor

Orientador: Michael John Brennan / Abstract: The guarantee of security in transport vehicles, buildings, bridges and critical structures is extremely important for people and the environment. Therefore, in the last decades, several Structural Health Monitoring (SHM) techniques have been proposed and developed for many areas. One technique to detect corrosion could be the use of guided waves. Considering one wave travelling in a structure and impinging on a discontinuity (damage), this wave will interact with this discontinuity and will be scattered. Thus wave motion in structures may be a powerful way to indicate the presence of damage in a structure. This work aims to investigate wave propagation in a thin Euler-Bernoulli infinite beam, and the way in which these waves interact with simulated corrosion damage (symmetric and asymmetric). The studies show the importance to know the behavior of waves before chose main frequencies to used for a SHM system. Piezoelectric elements are used to excite and sense the waves. The behavior of the systems studied are widely discussed in frequency and time domains. In order to detect and quantify the damage, reflected waves showed better sensitivity and proportionality with damage severity for all configuration studied. The longitudinal wave incident in the damage is easier to be used in a SHM system than flexural waves because longitudinal waves present simplicity compared to flexural. However, is important to choose appropriate frequency range in order to generate good levels of th... (Complete abstract click electronic access below) / Resumo: A garantia de segurança em veículos de transporte, edifícios, pontes e estruturas críticas é extremamente importante para as pessoas e o meio ambiente. Portanto, nas últimas décadas, várias técnicas de Monitoramento da Integridade Estrutural (SHM) foram propostas e desenvolvidas para diversas áreas. Uma técnica para detectar corrosão pode ser o uso de ondas guiadas. Considerando uma onda propaganda em uma estrutura e se chocando a uma descontinuidade (dano), esta onda irá interagir com esta descontinuidade e será transformada (parte é refletida e parte transmitida). Assim, o movimento de ondas em estruturas pode ser uma maneira poderosa de indicar a presença de dano em estruturas. Este trabalho tem como objetivo investigar a propagação de ondas em uma viga de Euler-Bernoulli e a forma como estas ondas interagem com danos simulados de corrosão (simétricos e assimétricos). Os estudos mostram a importância de conhecer o comportamento das ondas antes de escolher as freqüências principais a serem usadas em um sistema SHM. Elementos piezelétricos são usados para gerar sensoriar as ondas. O comportamento dos sistemas estudados é amplamente discutido nos domínios de frequência e tempo. Para detectar e quantificar os danos, as ondas refletidas apresentaram melhor sensibilidade e proporcionalidade com a severidade do dano para todas as configurações estudadas. As ondas longitudinais incidentes no dano são mais recomendadas pelo sistema SHM por apresentarem maior simplicidade em relação... (Resumo completo, clicar acesso eletrônico abaixo) / Doutor

Os pisos industriais são elementos que estão presentes em muitas obras da construção civil. Devido a isso, estudos devem ser procedidos para melhorar seu desempenho. Concretos reforçados com fibras metálicas são alternativas para a produção de pisos, pois as fibras melhoram o comportamento do concreto transformando-o de um material quase-frágil em um material com comportamento pseudo-ductil. Diversas manifestações patológicas vêm sendo constatadas em pisos, como fissuras, e o emprego destas fibras visa minimizar estas deficiências. Assim, nesta pesquisa, foi estudado o traço 1: 2,5: 3,1 a/c 0,55, com adição de três teores diferentes de fibras: 0,25%; 0,35% e 0,60%, em volume de concreto, e dois fatores de forma FF/65 e FF/80. Para avaliar características do concreto foram realizados ensaios de flexão a quatro pontos, flexão a três pontos, módulo de elasticidade e resistência à compressão axial. A partir destes ensaios pode-se verificar o comportamento de cada teor em relação: à tenacidade, às variações na carga de pico, à capacidade de manter a resistência residual pós-ruptura e à abertura da fissura. Também foram avaliadas as diferenças do comportamento em relação à moldagem dos CPs, devido ao fato que foram moldados CPs cilíndricos convencionais e extraídos de blocos. Verificou-se que a inserção de fibras não causa significativas alterações na resistência à compressão axial e também no módulo de elasticidade. Quando a análise é realizada para o tipo de moldagem verificou-se que os CPs cilíndricos convencionais obtiveram melhor desempenho, em comparação aos extraídos. Na avaliação dos ensaios de flexão observou-se que o teor exerce maior influência no desempenho se comparado com a mudança no fator de forma. padrão de fissuração nas vigas foi o esperado para teores abaixo do volume crítico. Verificou-se uma menor variabilidade dos resultados de flexão a três pontos em relação ao ensaio de flexão a quatro pontos. Constatou-se um aumento da energia de fratura com o aumento do teor de fibras. Com as propriedades estimadas experimentalmente foi dimensionado um piso industrial para uma aplicação específica, ressaltando que o teor de 0,35% seria a melhor alternativa. Concluindo que nesta pesquisa a variação no FF não causou impactos no desempenho final ressaltando que o teor de 0,35% seria a melhor alternativa, para o dimensionamento. / Industrial floors are elements that are present in many works of construction. Because of this, studies should be proceeded to improve their performance. Concrete reinforced with steel fibers are alternatives for the production of floors, because the fibers improve the concrete behavior making it a quasi-brittle material in a material with pseudo-ductile behavior. Several pathological manifestations have been observed in floors, such as cracks, and the use of these fibers is to minimize these deficiencies. Thus, in this research, we studied the trace 1: 2.5: 3.1 a / c 0.55, with addition of three different levels of fiber: 0.25%; 0.35% and 0.60% in volume of concrete, and two form factors FF / 65 and FF / 80. To evaluate specific characteristics of flexure tests were conducted at four points, the three points bending, modulus of elasticity and resistance to axial compression. From these tests can verify the behavior of each content regarding: the tenacity, to changes in peak load, the ability to maintain the post-break residual strength and the opening of the crack. They were also evaluated behavioral differences in relation to the molding of CPs due to the fact that were shaped conventional cylindrical CPs and extracted blocks. It was found that the fiber insertion does not cause significant changes in compressive strength and also the modulus of elasticity. When the analysis is performed for the type of molding it found that conventional cylindrical CPs performed better in comparison to extracted. In the evaluation of bending tests it was observed that the content has the most influence on performance compared with the change in form factor. The pattern of cracks on the beams was expected to levels below the critical volume. There was less variation of bending results at three points over the flexure test at four points. It was found an increased fracture energy with increased fiber content. With the properties estimated experimentally has been designed an industrial floor for a specific application, pointing out that the 0.35% level would be the best alternative. Concluding that this research variation in FF caused no impact on final performance pointing out that the 0.35% level would be the best alternative for the design.

Enquanto os métodos tradicionais de processamento de restaurações cerâmicas tornaram-se notórios por sua complexidade, as técnicas mais modernas vêm privilegiando a simplicidade de execução e a automação. Dentre estas, destaca-se a injeção em moldes, que recentemente, foi associada a métodos CAD-CAM. Estudos anteriores demonstraram a viabilidade de utilização de um vidro feldspático de baixa expansão térmica, Alpha (Vita Zahnfabrik), para injeção, porém, faltam informações quanto às propriedades mecânicas e a microestrutura deste material quando submetido à injeção. Os objetivos deste estudo são: produzir pastilhas vidrocerâmicas para injeção a quente a partir de Alpha e da mistura deste vidro com partículas de alumina e zircônia; avaliar a resistência à flexão dos materiais processados, e compará-la a um material compatível existente no mercado (PM9 - Vita Zahnfabrik); estudar a estrutura microscópica dos materiais e correlacioná-la com suas propriedades mecânicas; identificar por meio de difração de raios X a formação de fases cristalinas durante as diferentes etapas de processamento. A injeção aumentou a resistência do vidro Alpha devido à redução na quantidade e tamanho dos defeitos internos, principalmente porosidades. Apesar de ter sido observada nucleação de cristais nos dois materiais, durante o processamento, não foi possível determinar de que forma este fenômeno afetou as propriedades mecânicas dos materiais. Não foi detectada alteração no padrão de distribuição das fases cristalinas observadas em microscópio eletrônico de varredura antes e depois da injeção. Não foi verificada diferença estatística significante entre a resistência à flexão de Alpha injetado e PM9. A adição de partículas de alumina e zirconia ao vidro Alpha provocou redução da resistência, devido à formação de aglomerados durante a confecção das pastilhas e a incapacidade da injeção em dispersá-los. Tais aglomerados funcionaram como concentradores de tensões, enfraquecendo o material. / While traditional processing routes in the fabrication of ceramic restorations became notorious for their complexity, modern techniques have been priviledging simplicity and automation. High-temperature injection molding is a clear example, and recently has been associated to CAD-CAM technology. Studies demonstrated the use of a low thermal expansion feldspathic glass (Alpha, Vita Zahnfabrik) for injection, although more information is needed in terms of mechanical properties and microstructure of this material after being submitted to injection. The objectives of this study are: produce Alpha glass-ceramic ingots and Alpha with alumina and zirconia particles ingots for injection; evaluate flexural strength of the processed materials and compare it to a compatible product (PM9-Vita Zahnfabrik); study microstructure of the materials and correlate it to their mechanical properties; identify the existing cristalline phases at different processing stages with X-ray diffraction. Injection increased mechanical properties of Alpha glass due to reduction in porosity of the material. Despite the observation of crystal nucleation on both materials during processing, a clear correlation of this phenomenon and mechanical behavior could not be made. No alterations on the pattern of the crystalline phase distribution due to injection were observed on scanning electron microscope images. Flexural strength did not vary significantly between injected Alpha and PM9. The addittion of alumina and zirconia particles resulted in poorer mechanical results due to agglomerate formation during ingot fabrication and the incapacity of its dispersion trough injection. These agglomerates worked as stress concentrators, weakening the material.

Failure criteria play a vital role in the numerical analysis of reinforced concrete structures. The current failure criteria can be classified into two types, namely the empirical and theoretical failure criteria. Empirical failure criteria normally lack reasonable theoretical backgrounds, while theoretical ones either involve too many parameters or ignore the effects of intermediate principal stress on the concrete strength. Based on the octahedral shear stress model and the concrete tensile strength under the state of triaxial and uniaxial stress, a new failure criterion, that is, the simplified unified strength theory (UST), is developed by simplifiing the five-parameter UST for the analysis of reinforced concrete structures. According to the simplified UST failure criterion, the concrete strength is influenced by the maximum and intermediate principal shear stresses together with the corresponding normal stresses. Moreover, the effect of hydrostatic pressure on the concrete strength is also taken into account. The failure criterion involves three concrete strengths, namely the uniaxial tensile and compressive strengths and the equal biaxial compressive strength. In the numerical analysis, a degenerated shell element with the layered approach is adopted for the simulation of concrete structures. In the layered approach, concrete is divided into several layers over the thickness of the elements and reinforcing steel is smeared into the corresponding number of layers of equivalent thickness. In each concrete layer, three-dimensional stresses are calculated at the integration points. For the material modelling, concrete is treated as isotropic material until cracking occurs. Cracked concrete is treated as an orthotropic material incorporating tension stiffening and the reduction of cracked shear stiffness. Meanwhile, the smeared craclc model is employed. The bending reinforcements and the stirrups are simulated using a trilinear material model. To verify the correctness of the simplified UST failure criterion, comparisons are made with concrete triaxial empirical results as well as with the Kupfer and the Ottosen failure criteria. Finally, the proposed failure criterion is used for the flexural analysis of simply supported reinforced concrete beams. Also conducted are the punching shear analyses of single- and multi-column-slab connections and of half-scale flat plate models. In view of its accuracy and capabilities, the simplified UST failure criterion may be used to analyse beam- and slab-type reinforced concrete structures.

Aluminum alloys are having more attention due to their high specific stiffness and processing advantages. 7075 aluminum alloy is a wrought composition aluminum alloy in the Al-Zn-Mg-Cu series. Due to the significant addition of these alloying elements, 7075 has higher strength compared to all other aluminum alloys and effective precipitation hardenability characteristic. On the other hand, aluminum alloys have some drawbacks, which hinder the widespread application of them. One of the most commonly encountered defects in aluminum alloys is the hydrogen porosity. Additionally, in case of 7075, another problem is the lack of fluidity. Magnesium addition is thought to be effective in compensating this deficiency. Accordingly, in this study, die cast 7075 aluminum alloy samples with hydrogen porosity and additional magnesium content were investigated. The aim was to determine the relationship between hydrogen content and hydrogen porosity, and the effects of hydrogen porosity, additional magnesium and T6 heat treatment on ultimate tensile and flexural strength properties of pressure die cast 7075 aluminum alloy. 7075 aluminum alloy returns were supplied from a local pressure die casting company. After spectral analysis, pressure die casting was conducted at two stages. In the first stage, 7075 aluminum alloy with an increase in magnesium concentration was melted and secondly 7075 aluminum alloy was cast directly without any alloying addition. While making those castings, hydrogen content was measured continuously before each casting operation. As a final operation T6 heat treatment is carried out for certain samples. Finally, in order to accomplish our aim, mechanical and microstructural examination tests were conducted.

Wood Plastic Composites (WPC) have advantages over natural wood such as improved stiffness, recyclability, and waste minimization. However, issues such as the difficulty of processing WPC with conventional methods, volatile emission from the wood and the composites’ lack of strength must be addressed. A system for continuous extrusion of rectangular profiles of WPC was developed and some critical processing strategies were identified. The use of a lubricant and a calibrator also improved the profile extrusion of WPC. In this work, glass was also added to improve WPC’s mechanical strength. Generally, a glass content of 2.5% appears to improve the properties but further addition does not have a significant effect. Foaming of WPC, which can enhance their properties, was investigated through studying the effect of heating time and temperature on void fraction and cell density. / UOIT

Preparation of thermoplastics composites using engineering thermoplastics and plant fibers or fillers is a technical challenge because the processing temperature of the thermoplastics is generally above the temperature of degradation of plant fibers of fillers. There have been numerous attempts for processing high melting point engineering thermoplastics like Nylon-6 with plant natural fibers and fillers. Low temperature processing methods, fiber modification or addition of additives which drops polymer melting point are some of proposed solutions for this problem. The objective of this thesis was to develop a formulation using wheat straw (WS) as a reinforcing fiber for Nylon-6. The concentration of WS was 15 wt-%. The thermoplastic composites were prepared by mixing grinded wheat straw and Nylon-6 using a laboratory scale twin-screw extruder; follow by preparation of samples using injection moulding. The strategy investigated in this thesis was utilization of additives to lower the melting point or to decrease the viscosity of Nylon-6. Lithium chloride salt (LiCl) and N-Butyl benzene Sulfon amide plasticizer (N-BBSA) were used as process additives to decrease melting point and to reduce the processing temperature and time. The addition of the wheat straw (15 wt-%) to the Nylon-6 increased modulus by 26.9 % but decreased the strength by 9.9 %. Effect of different level of these two additives on mechanical, thermal, physical properties and processability of the composite runs were studied. Addition of 4 wt-% LiCl was found to decrease the melting point from 222 °C to 191 °C, to increase modulus by 14 % in comparison to Nylon-6/wheat straw (15 wt-%). However, it decreased the processability and strength by 12.7 %. Plasticizer was investigated to easing processability and decreasing the degradation by reducing the residence time in the extruder, it does not affect the melting point of Nylon-6. The addition of 4 wt-% of plasticizer (N-BBSA) increased modulus and strength only by 2.6 % and 3 %, respectively, in comparison to Nylon-6/wheat straw (15 wt-%) composites. The results of mechanical properties were used as a benchmark for comparisons among samples with different formulations (levels of additives) to find out levels of LiCl and N-BBSA for the best mechanical properties. It was found that samples with 2 wt-% LiCl and 2 wt-% of N-BBSA had 29.3 % higher tensile modulus than neat Nylon-6, while its strength was almost same as neat Nylon-6 and 6.3 % higher than Nylon-6/WS (15 wt-%). These results were used to correlate the mechanical properties as a function of percentage of salt and plasticizer in the formulation. Differential scanning calorimetry (DSC) was used to evaluate the percentage of crystallinity and the melting point of the thermoplastic phase and thermal gravimetric analysis (TGA) was used to measure the thermal stability of different formulation. The kinetics of crystallization and degradation were evaluated using results from DSC and TGA, respectively. The activation energy for thermal degradation and the percentage of crystallinity of the thermoplastic composites were correlated to mechanical properties using linear regression. It was found that fiber degradation had a significant effect on strength but the effects of percentage of crystallinity on composites strength were insignificant. On the other hand, the percentage of crystallinity affects stiffness and impact strength. The ductility was a function of both crystallinity and thermal stability.